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Development of a qualitative liquid chromatography/tandem mass spectrometric method for the detection of narcotics in urine relevant to doping analysis.
Rapid Commun Mass Spectrom. 2007; 21(18):3015-23.RC

Abstract

A new screening procedure for 18 narcotics in urine for anti-doping purposes has been developed using liquid chromatography/triple quadrupole mass spectrometry (LC/MS). Electrospray ionization (ESI) was used as interface. Infusion experiments were performed for all substances to investigate their mass spectrometric behaviour in terms of selecting product specific ions. These product ions were then used to develop a tandem mass spectrometric method using selected reaction monitoring (SRM). For the LC/MS analysis, chromatography was performed on an octadecylsilane column. The total run time of the chromatographic method was 5.5 min. For the sample preparation prior to LC/MS analysis, the urine samples were liquid-liquid extracted at pH 9.5 after overnight enzymatic hydrolysis. Two extraction solvents were evaluated: dichloromethane/methanol 9/1 (v/v), which is currently used for the extraction of narcotics, and diethyl ether, used for the extraction of steroids. With diethyl ether the detection limits for all compounds ranged between 0.5 and 20 ng/mL and with the mixture containing dichloromethane the detection limits ranged between 0.5 and 10 ng/mL. Taking into account the minimum required performance limits of the World Anti-Doping Agency of 200 ng/mL for narcotics, diethyl ether can also be considered as extraction solvent for narcotics. Finally, the described method was applied to the analysis of urine samples previously found to contain narcotics by our routine gas chromatography/mass spectrometry (GC/MS) method.

Authors+Show Affiliations

Ghent University (UGent), Department of Clinical Chemistry, Microbiology and Immunology, Doping Control Laboratory (DoCoLab), Technologiepark 30, B-9052 Zwijnaarde, Belgium. Koen.Deventer@UGent.beNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Evaluation Study
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17708509

Citation

Deventer, Koen, et al. "Development of a Qualitative Liquid Chromatography/tandem Mass Spectrometric Method for the Detection of Narcotics in Urine Relevant to Doping Analysis." Rapid Communications in Mass Spectrometry : RCM, vol. 21, no. 18, 2007, pp. 3015-23.
Deventer K, Pozo OJ, Van Eenoo P, et al. Development of a qualitative liquid chromatography/tandem mass spectrometric method for the detection of narcotics in urine relevant to doping analysis. Rapid Commun Mass Spectrom. 2007;21(18):3015-23.
Deventer, K., Pozo, O. J., Van Eenoo, P., & Delbeke, F. T. (2007). Development of a qualitative liquid chromatography/tandem mass spectrometric method for the detection of narcotics in urine relevant to doping analysis. Rapid Communications in Mass Spectrometry : RCM, 21(18), 3015-23.
Deventer K, et al. Development of a Qualitative Liquid Chromatography/tandem Mass Spectrometric Method for the Detection of Narcotics in Urine Relevant to Doping Analysis. Rapid Commun Mass Spectrom. 2007;21(18):3015-23. PubMed PMID: 17708509.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development of a qualitative liquid chromatography/tandem mass spectrometric method for the detection of narcotics in urine relevant to doping analysis. AU - Deventer,Koen, AU - Pozo,Oscar J, AU - Van Eenoo,Peter, AU - Delbeke,Frans T, PY - 2007/8/22/pubmed PY - 2007/11/14/medline PY - 2007/8/22/entrez SP - 3015 EP - 23 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 21 IS - 18 N2 - A new screening procedure for 18 narcotics in urine for anti-doping purposes has been developed using liquid chromatography/triple quadrupole mass spectrometry (LC/MS). Electrospray ionization (ESI) was used as interface. Infusion experiments were performed for all substances to investigate their mass spectrometric behaviour in terms of selecting product specific ions. These product ions were then used to develop a tandem mass spectrometric method using selected reaction monitoring (SRM). For the LC/MS analysis, chromatography was performed on an octadecylsilane column. The total run time of the chromatographic method was 5.5 min. For the sample preparation prior to LC/MS analysis, the urine samples were liquid-liquid extracted at pH 9.5 after overnight enzymatic hydrolysis. Two extraction solvents were evaluated: dichloromethane/methanol 9/1 (v/v), which is currently used for the extraction of narcotics, and diethyl ether, used for the extraction of steroids. With diethyl ether the detection limits for all compounds ranged between 0.5 and 20 ng/mL and with the mixture containing dichloromethane the detection limits ranged between 0.5 and 10 ng/mL. Taking into account the minimum required performance limits of the World Anti-Doping Agency of 200 ng/mL for narcotics, diethyl ether can also be considered as extraction solvent for narcotics. Finally, the described method was applied to the analysis of urine samples previously found to contain narcotics by our routine gas chromatography/mass spectrometry (GC/MS) method. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/17708509/Development_of_a_qualitative_liquid_chromatography/tandem_mass_spectrometric_method_for_the_detection_of_narcotics_in_urine_relevant_to_doping_analysis_ L2 - https://doi.org/10.1002/rcm.3142 DB - PRIME DP - Unbound Medicine ER -